悬浮液进样端视电感耦合等离子体发射光谱法直接测定二氧化钛中铌

用聚丙烯酸胺(NH₄PAA)为分散剂制备二氧化钛悬浮液,并以悬浮液进样端视电感耦合等离子体发射光谱法直接测定了二氧化钛中痕量杂质铌。研究了分散剂及分散剂的量和pH对二氧化钛悬浮液稳定性的影响,通过优化条件制备得到稳定和均匀的悬浮液。研究了端视电感耦合等离子体发射光谱分析悬浮液进样的性能。本方法的检出限为3.0 μg·L-1, 相对标准偏差为3.1%(n=3, c=0.3 mg·L-1)。     

丙二醇甲醚中超痕量金属杂质元素的ICP-MS/MS分析

基于电感耦合等离子体串联质谱(ICP-MS/MS)建立了准确测定丙二醇甲醚中超痕量金属杂质元素的分析方法,提出了利用混合反应气消除质谱干扰的新策略.丙二醇甲醚经超纯水稀释后直接采用IC P-MS/MS测定其中具有挑战性的超痕量金属元素Mg,Al,K,Ti,V,Cr,Fe,Ni,Cu和Zn,在MS/MS模式下,选择混合气...     

Zhp-2型火花源固体双聚焦质谱仪

一、引 言 Zhp-2型火花源固体双聚焦质谱仪,是一种利用离子光学方法分析固体样品中微量杂质元素的大型仪器.它在物理学研究和应用工作中起着越来越重要的作用. 随着近代科学技术的发展,新材料的应用越来越广泛.对超纯物质的纯度提出越来越高的要求.如半导体材料中某些微量杂质的存在,足以影响材料及器件的重要性能.因此,在生产工艺上必须加以控制,要求相对灵敏度达到 10-8-10-10,甚至更高. 迄今为止,具有较高灵敏度的分析手段有发射光谱法、原子吸收分光光度法、原子荧光法、质谱分析法以及活化分析法,等等.其中以活化分析、无火焰原子吸收…     

电感耦合等离子体质谱法进样技术研究

电感耦合等离子体质谱(ICP-MS)是近年发展起来的新型痕量元素分析技术,可以用于检出限为pg/ml级的痕量元素及天然同位素分析,同位素比分析及常规同位素稀释质谱分析等。所有这些应用都显示出ICP-MS在痕量元素分析领域中具有无与伦比的优点。ICP-MS进样技术一直是人们所关注的     

电感耦合等离子体发射光谱法测定E10乙醇汽油中的钠和锌

车用乙醇汽油是一种新型、清洁的汽车燃料,在燃烧过程中,微量的重金属杂质对汽车的行驶和养护有着至关重要的影响,一些燃烧产物可能会污染环境,威胁人们的身体健康,因此有必要对其中的微量元素进行控制.以异辛烷稀释汽油样品,电感耦合等离子体发射光谱(IC P-O ES)法测定车用E10乙醇汽油中钠、锌含量的方法,选择钠和锌的分析...     

大气压冷等离子体喷枪气体温度的比较研究

采用介质阻挡放电等离子体喷枪装置,在大气压下流动气体(氩气和痕量氮气)中产生了稳定的喷射等离子体.通过拍摄喷枪发光照片,研究了喷射等离子体长度随气体流量的变化关系.利用高分辨率光谱仪采集等离子体羽处的发射光谱,通过对发射光谱中N+2的第一负系(B 2Σ+u→X 2Σ+g,390～391.6 nm)谱线拟合得到了射流等离...     

Kalman滤波法在电感耦合等离子体原子发射光谱分析中的应用 Ⅰ．测定高纯氧化铥中的14种稀土杂质

本文研究了电感耦合等离子体原子发射光谱分析Ｋａｌｍａｎ滤波法测定高纯氧化铥中的１４种其他稀土杂质的方法。Ｋａｌｍａｎ滤波法有效地消除光谱干扰，可利用受干扰的光谱灵敏线，因而可提高灵敏度，是一种在大量基体存在下测定痕量杂质的有效方法。     

Kalman滤波法在电感耦合等离子体原子发射光谱分析中的应用──Ⅱ．测定高纯氧化铕中的14种稀土杂质

本文研究了电感耦合等离子体原子发射光谱分析Ｋａｌｍａｎ滤波法测定高纯氧化铕中的１４种其他稀土杂质的方法。Ｋａｌｍａｎ滤波法有效地消除光谱干扰，可利用受干扰的光谱灵敏线，因而可提高灵敏度，是一种在大量基体存在下测定痕量杂质的有效方法。     

Kalman滤波法在电感耦合等离子体原子发射光谱分析中的应用…

本文研究了电感耦合等离子体原子发射光谱分析Ｋａｌｍａｎ滤波法测定高纯氧化铕中的１４种其他稀土杂质的方法。Ｋａｌｍａｎ滤波法有效地消除光谱干扰，可利用受干扰的光谱灵敏线，因而可提高灵敏度，是一种在大量基体存在下测量痕量杂质的有产方法。     

悬浮液雾化进样感耦等离子体基本参数研究——Ⅱ等离子体电子密度测定

研究了悬浮液雾化进样感耦等离子体原子发射光谱基本参数-等离子体电子密度的测定。实验使用Stark效应常用的谱线H_β线来计算等离子体电子密度。测定结果表明悬浮液雾化进样同水溶液雾化进样感耦等离子体原子发射光谱时等离子体电子密度没有发生显著的变化,数值基本上为1015数量级。固含量高达10％ TiO₂悬浮液雾化进样等离子体原子发射光谱,电子密度测定结果仅有微小的降低。高固含量悬浮液雾化进样等离子体原子发射光谱没有显著地影响等离子体电子密度,有助于使用高固含量悬浮液雾化进样等离子体原子发射光谱来进行痕量元素分析测定。     

Yttria tetragonal zirconia polycrystalline electrolytes for solid state electrochemical cells

Both the grain-boundary and the lattice resistivity in Y-TZP materials is affected by several ceramic processing variables. These include, sintering temperature, sintering time, cooling rate from high temperatures (>1000°C), post-sinter heat treatments, the level and types of impurities and the spatial distribution of Y₂O₃ in the starting powders. Because of the inherent large grain-boundary surface area the grain-boundary resistivity in these ceramics is extremely sensitive to the presence and location of glassy impurities. Impedance spectroscopy has been used along with four-probe dc conductivity measurements, scanning and transmission electron microscopy, x-ray photoelectron spectroscopy and x-ray diffraction to understand the grain-boundary and lattice resistivity behaviour in Y-TZP ceramics as a function of various ceramic processing variables.     

Effect of grain boundaries on the conductivity of high-purity ZrO2Y2O3 ceramics

Grain boundary conductivities are determined by complex impedance measurements (1–10⁶ Hz) on high-purity ceramics prepared by the alkoxide synthesis and on less pure ceramics obtained from a commercial powder. The grain size was varied systematically in the region 0.36–55 μm. The grain boundary conductivity is strongly influenced by the grain size, impurities and cooling procedure. The grain boundary conductivity increases linearly with the grain size for small grain sizes (0.3 to 2–4 μm) and is constant for larger grain sizes. The calculated specific conductivity of the grain boundary for pure materials is about 100 times smaller than that of the bulk. The grain boundary thickness was estimated to be 5.4 nm. The activation energy of the grain boundary conductivity is 7 kJ mole^?1 higher than of the bulk.     

Al-26 diffusion measurement in 2/1-mullite by means of Secondary Ion Mass Spectrometry

Aluminium is an important constituent of advanced structural and functional ceramics, as well as of geological materials in the upper mantle. Aluminium has only one single stable isotope and radioisotopes which are difficult to apply routinely in radiotracer diffusion experiments. Therefore, it is a methodological challenge to measure aluminium diffusivities. Our novel approach consists in using the long-life radioactive isotope ²⁶Al as a pseudo-stable isotope whose depth distribution can be analysed with Secondary Ion Mass Spectrometry after a diffusion experiment. For our demonstration we chose mullite (Al_4+2xSi_2−2xO_10−x, 0.2< x < 0.5) which is an important candidate for advanced structural and functional ceramics with some outstanding properties: low thermal expansion, low thermal conductivity, and excellent creep resistance. The method is universally applicable to the huge family of aluminium containing oxides.     

Model Studies of Rayleigh Instabilities via Microdesigned Interfaces

The energetic and kinetic properties of surfaces play a critical role in defining the microstructural changes that occur during sintering and high-temperature use of ceramics. Characterization of surface diffusion in ceramics is particularly difficult, and significant variations in reported values of surface diffusivities arise even in well-studied systems. Effects of impurities, surface energy anisotropy, and the onset of surface attachment limited kinetics (SALK) are believed to contribute to this variability. An overview of the use of Rayleigh instabilities as a means of characterizing surface diffusivities is presented. The development of models of morphological evolution that account for effects of surface energy anisotropy is reviewed, and the potential interplay between impurities and surface energy anisotropy is addressed. The status of experimental studies of Rayleigh instabilities in sapphire utilizing lithographically introduced pore channels of controlled geometry and crystallography is summarized. Results of model studies indicate that impurities can significantly influence both the spatial and temporal characteristics of Rayleigh instabilities; this is attributed at least in part to impurity effects on the surface energy anisotropy. Related model experiments indicate that the onset of SALK may also contribute significantly to apparent variations in surface diffusion coefficients.     

敏感半导体陶瓷的显微物理模型(Ⅱ)

本文用敏感半导体陶瓷的显微物理模型描述了热敏、气敏和湿敏陶瓷的电性能。得到了一些重要的结果。这些理论结果与实验结果相符,它们为敏感陶瓷的设计提供了理论依据。可预料该模型可作为这类半导体陶瓷的统一的显微物理模型。 关键词：     

Short-Circuit Diffusion in Ceramics

This article discusses grain boundary diffusion in ceramics. It gives a brief review of the experimental data available for ionic oxides and the problems of interpretation associated with it. The fundamental differences between grain boundary diffusion in metals and ceramics are noted. Calculations of the segregation of defects and impurities to grain boundaries are discussed together with methods of calculating diffusion coefficients in these boundaries. New results for alumina and chromia are presented. The problem of defining a grain boundary width is discussed with respect to new calculations on nickel oxide.     

Magnetic properties of lithium intercalation compounds

Magnetic experiments are powerful tools to study fundamental properties and to check the qualities of samples. Temperature, stress, and impurities of materials can all affect magnetic properties and play an important role in the utilization of these materials for engineering applications. The estimation and analysis of the spontaneous magnetization can reveal ferromagnetic particles as impurities in samples. The shape of the temperature dependence of magnetization is indicative of the origin of the magnetic properties. However, it is necessary to correlate the χ _m (T) curves and isothermal M(H) plots to achieve a complete analysis of the electronic properties of the materials. Highlights of magnetic properties of lithium intercalation compounds are briefly described. Intrinsic and extrinsic properties are considered as useful parameters to determine the purity of electrode materials for rechargeable Li-ion batteries.     

激光剥蚀-电感耦合等离子体质谱法测定高纯铪中10种杂质元素

高纯铪由于具有独特的理化性质,在核反应堆、等离子切割机、光学元件等方面有着重要的应用。高纯铪中杂质的种类和含量会影响高纯铪的物理化学性能,应用中对高纯铪纯度的要求也越来越高,这就对高纯铪的分析检测技术提出了更高的要求。激光剥蚀-电感耦合等离子体质谱法（LA-ICP-MS）是激光剥蚀进样技术与电感耦合等离子体质谱联用,可以直接分析固体样品,并且方法前处理简单,可以避免样品前处理过程中引入杂质,是一项高效、快速、精密的分析技术,在环境、地质、冶金、燃料能源、材料、生物医药、考古等领域广泛应用。所以,激光剥蚀-电感耦合等离子体质谱法（LA-ICP-MS）是高纯金属杂质元素最佳检测方法之一。还未见有应用LA-ICP-MS于高纯铪样品的报道。用LA-ICP-MS对高纯铪中10种杂质元素（Al,Sc,Ti,Fe,Ni,Cu,Mo,Ag,Sn,W）进行定量分析。为了降低激光剥蚀过程中元素的分馏效应,提高信号灵敏度和稳定度,对激光剥蚀参数进行优化实验。确定了激光剥蚀的最优仪器参数为：氦气流量600 mL·min-1,激光能量90%,剥蚀孔径150 μm,激光扫描速度60 μm·s-1,激光脉冲频率20 Hz。经实验优化后的ICP-MS仪器工作参数为：RF功率1 450 W,射频匹配电压1.8 V,载气流量0.85 L·min-1,冷却器流量0.85 L·min-1,采样深度7.5 mm。在最优参数条件下,利用内控标样建立工作曲线,各杂质元素标准曲线的线性相关系数为0.993 6～0.999 8。采集载气空白的信号强度,平行测定11次,以3倍空白信号的标准偏差所对应的含量作为元素的检出限,得到各元素的检出限为0.001~0.08 μg·g-1。将高纯铪制成尺寸合适的样品,用硝酸洗去样品表面的氧化物,将其装入剥蚀池中,运用线扫描剥蚀方式,在最佳仪器工作条件下,对三个高纯铪样品中的10种杂质元素进行定量分析。实验结果显示,杂质元素含量为0.17～36.76 μg·g-1,相对标准偏差为1.4%～20%,精密度良好。以184W为例,将LA-ICP-MS法和ICP-MS法的测定结果进行t检验,三个样品的t值分别为2.14,1.64和2.11,均小于显著性水平为0.05时的临界值（t_{0.05, 12}=2.18）,说明LA-ICP-MS法和ICP-MS法的测定结果在置信度为95%时没有显著性差异,即正确度良好。所以,该方法正确度和精密度良好,可用于高纯铪中杂质的定量分析。     

Crystal quality boosts responsiveness of magnetic shape memory single crystals

Magnetic shape memory alloys are promising materials to replace giant magnetostrictive materials and piezoelectrical ceramics in actuating devices due to the large magnetically induced strains. Ni-Mn-Ga is the most intense studied system due to its relatively high operational temperatures and the huge magnetically induced strains reported. Up to now the application of these materials is still limited by the operational temperature range. Additionally twin boundary mobility suffers from structural defects increasing the magnetic fields needed for significant and reproducible strains. The sample quality is affected by crystal inhomogeneity, porosity and impurities. Here new results are reported for the Ni-Mn-Ga class based on a set of single crystals grown by the SLARE method, recently developed by Mecklenburg et al. Single crystalline samples of Ni_49.7Mn_29.3Ga₂₁ of tetragonal martensitic structure exhibit a magnetic field induced strain of more than 4% below 170 mT and 6.5% at only 340 mT. Furthermore the operational temperature regimen could be expanded up to 65 °C.     

用X射线荧光光谱法测定钢材中成份

钢材是以铁为基体的多元体系。本方法采用X荧光光谱测定钢材中的元素成份,除测定杂质元素外并能测定基体元素铁。测定结果是令人满意的。